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3.7 Experimental 3.7.1 General Methods All chemical reagents were used without further purification. Solvents for column chromatography and TLC were laboratory grade and distilled before use. For thinlayer chromatography (TLC), analytical TLC plates (Alugram SIL G/UV254 (E. M. Merk) were used. Column chromatography was performed with flash silica gel (100- 200 mesh) or neutral alumina oxide (50-200 micron). 1 H and 13 C NMR spectra were recorded on a Bruker Avance 300 (300 MHz) or a Bruker AMX-400 (400 MHz) spectrometers. NMR samples were run in the indicated solvents and were referenced internally. Chemical shift values were quoted in ppm and coupling constants were quoted in Hz. Chemical shift multiplicities were reported as s = singlet, d = doublet, t = triplet, q = quartet, m = multiplet and br = broad. Low-resolution mass spectra were recorded on a HEWLETT-PACKARD instrument (CI or EI) and LCQ Advantage instrument (ESI). High-resolution mass spectra (EI) were recorded on a KRATOS MS50TC instrument. Melting points were determined using Reichert-Jung Thermovar apparatus and were uncorrected. 3.7.2 Microwave Irradiation Experiments Microwave irradiation experiments were carried out in a dedicated CEM-Discover mono-mode microwave apparatus or Milestone MicroSYNTH multi-mode microwave reactor (Laboratory Microwave Systems). Microwave apparatuses were used in the standard configuration as delivered, operating at a frequency 2.45 GHz with continuous irradiation power from 0 to 400 W. The reactions were carried out in 10, 20, 30 and 50 mL glass tubes. The temperature was measured with an IR sensor on the outer surface of the process vial or fibre optic sensor inside the process vial. After the irradiation period, the reaction vessel was cooled rapidly (2-5 min) to ambient temperature by air jet cooling.
3.8. Experimental protocols 3.8.1 General Procedure for the Preparation of hydroxy Salts. (Microwave) According to process described in chapeter-2 40 new hydrocy salts were synthesized 3.8.2 General Procedure for the Preparation of HClO4 Salts. A mixture of 84% polyphosphoric acid (3 g) and hydroxy salts (3 mmol) was heated in 50 ml beaker upon intensive stirring at 150 °C for 15 min. After cooling to the room temperature the resulting viscous mass was dissolved in 30 ml of water and 1 ml (10 mmol) of 70% HClO4 was added dropwise upon mild stirring. The white precipitate was washed with distilled water (3×10 mL), ether (2×10 mL) until a neutral reaction of the pH paper and then dried over P2O5 to give salt as fine white crystals. In similar manner 40 new compounds were synthesized. 3.8.3 General Procedure for the Microwave-Assisted Synthesis of 2aminoimidazoles. To a suspension of HClO4 salt (2 mmol) in MeCN (5 mL) hydrazine hydrate (0.7 mL, 14 mmol of a 64% solution, 7 equiv) was added, and the mixture was irradiated in the sealed Milestone MicroSYNTH microwave reactor for 10 min at a ceiling temperature of 100 °C at 150 W maximum power. After cooling down the reaction was worked up by diluting with DCM (300 mL), washing with sat. NH4Cl solution (150 mL), brine (150 mL) and water (2×150 mL) and drying over anhydrous Na2SO4. After filtration and concentration the resulting residue was purified by column chromatography (silica gel; DCM−MeOH, 9:1 v/v with 3% TEA) to afford the product as a colourless solid. 40 new compounds were synthesized In similar manner.
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Saurashtra University Re - Accredit
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JANUARY-2011 Statement under O. Ph.
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Acknowledgment This thesis arose in
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since I was a child. My Mother Hans
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CHAPTER - 2 Microwave Assisted Synt
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5.5 Results and discussion 156 5.6
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Ms Mesyl MW Microwave NBS N-bromosu
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1. Microwave Assisted Organic Synth
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1.4 Heating Mechanism In microwave
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1.5. Effects of solvents Every solv
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1.7 Application of microwave in org
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aromatic amines, Lancini’s group
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1.9 2-Aminoimidazole Alkaloids The
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Recently group of Erik 83 described
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1.10 Methods for the preparation of
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R 1 O X R 2 NH 2 H 2N NAc R 1 HN R
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this manifold, was reported in 1925
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Another route to 4(5)-acyl-2-amino-
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this series of compounds against th
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documented. Extra care is needed be
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Very recently the research group of
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OH a,b O N H2N N Boc N 3 H N R N N
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1.12.2 Biofilm Growth Cycle 1) Plan
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can survive both the onslaught of a
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[26] Leadbeater, N. E. (2004) Chemi
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[86] Kreutzberger, A. (1962) J. Org
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Microwave Assisted Synthesis & Stru
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2.1 Introduction As described in ch
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2.3 Proposed Mechanism: Regarding t
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No. 12 60 120 traces 84 a All react
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the development of biofilm related
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In first instance, a series of 2-hy
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Br N N N R 1 OH Br N N N R 1 OH Fig
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Page 71 and 72: 2.6 Conclusion In the present study
Page 73 and 74: 2.8 Biological assays 2.8.1 Static
Page 75 and 76: 2.9 Experimental protocol: 2.9.1 Ge
Page 77 and 78: temperature of 80 °C and a maximum
Page 79 and 80: 29.5,29.4, 29.2, 27.0, 22.6, 14.1.
Page 81 and 82: Yield: 78 %. 1 H NMR (300 MHz, CDCl
Page 83 and 84: N Br N N C 14H 29 OH Yield: 72 %. 1
Page 85 and 86: (75.5 MHz, CDCl3): δ = 167.7, 154.
Page 87 and 88: N Br N N C 14H 29 OH Cl Yield: 90 %
Page 89 and 90: 2-(3,4-Dichlorophenyl)-2-hydroxy-1-
Page 91 and 92: N Br N N C 8H 17 OH NO 2 Yield: 49
Page 93 and 94: C3H7 HN N N H Cl Cl Yield : 70 %. 1
Page 95 and 96: (s, 1H), 3.16 (s, 3H), 1.80 (m, 2H)
Page 97 and 98: 5-(4’-Nitrobiphenyl-4-yl)-N-octyl
Page 99 and 100: 2.11 Representative NMR spectra 2.1
Page 101 and 102: 2.11.3 10.4329 0.7429 151.5720 10.0
Page 103 and 104: [21] Matz C, McDougald D, Moreno A.
Page 105 and 106: Chapter-3 Structure Activity Relati
Page 107 and 108: imidazoles, where the addition of a
Page 109 and 110: 3.4 Result and Discussion It was fo
Page 111 and 112: No. H 2N Compound Code N N C8H17 R1
Page 113 and 114: medium used in the set-up to monito
Page 115 and 116: H 2N N N N H2N N R R Figure-1 Effec
Page 117 and 118: 3.5.3 Cyclo-alkyl 2-aminoimidazoles
Page 119: 3.6. Conclusion In the present stud
Page 123 and 124: 122.6, 54.6, 33.3(×2), 27.3 (×2),
Page 127 and 128: 5-(4-Chlorophenyl)-1-cyclooctyl-1H-
Page 129 and 130: Yield: 50 %. Mp: 76-78 ° C. 1 H NM
Page 131 and 132: 5-(4-Chlorophenyl)-1-cyclobutyl-1H-
Page 133 and 134: Yield: 66%. 1 H NMR (300 MHz, CDCl3
Page 135 and 136: 3.10 Representative NMR spectra 3.1
Page 137 and 138: 3.11 References [1] (a) Alvi K. A,
Page 139 and 140: Copper Catalyzed Microwave Assisted
Page 141 and 142: 4.1 Introduction There are only a f
Page 143 and 144: (Table-1, No- 6). Next reaction tem
Page 145 and 146: No. Product, Yield b (%) No. Produc
Page 147 and 148: 4.4 Possible Mechanism Regarding th
Page 149 and 150: 4.7 Experimental protocols 4.7.1 Ge
Page 153 and 154: 1-(3-Azidopropyl)-2-(3,4-dichloroph
Page 155 and 156: Yield: 84 %. 1 H NMR (300 MHz, DMSO
Page 161 and 162: 1H), 1.66 (m, 6H), 1.70 (m, 2H). 13
Page 163 and 164: 5.48 Hz, 2H), 3.59 (m, 2H), 3.16 (d
Page 165 and 166: 4.10 References [1] For a general r
Page 167 and 168: Crystal and Molecular Structure Ana
Page 169 and 170: 5.1 Introduction The membrane efflu
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oscillation range of 5˚ and proces
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C12-C13 1.372(4) C32-C37 1.390(3) C
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Fig.-3: Packing of the molecules wh
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1 H NMR (400 MHz CDCl3): δ = 7.57-
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5.9.2 13 C spectra of bs-DP-7
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SUMMARY The work represented in the
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CONFERENCES/SEMINARS/WORKSHOPS ATTE
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PUBLICATIONS [1] One-Pot Microwave-
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Scheme 2 Competitive formation of 1
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Table 2 continued 9 10 11 12 N hydr
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8. Colson G, Raboult L, Lavelle F,
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